High-Speed Liquid Chromatographic Determination of Biphenyl Residues in Citrus Products

1975 ◽  
Vol 58 (5) ◽  
pp. 1013-1014
Author(s):  
Samuel K Reeder

Abstract A simple, direct, and rapid method is given for the analysis of citrus oils for the fungistat biphenyl by high-speed liquid chromatography. The method is extended to orange juice and various “dry flavors” by an extraction procedure. Analytical limits are <1 ppm without need for any cleanup or concentration steps.

1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


1984 ◽  
Vol 67 (6) ◽  
pp. 1135-1137 ◽  
Author(s):  
Yoshiki Onji ◽  
Masakiyo Uno ◽  
Tanigawa Kaoru

Abstract A simple and rapid method was developed for quantitative determination of common tetracyclines, such as oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC), in meat and fish. Tetracyclines were extracted with aqueous HCI, and then centrifuged. The supernate was applied to an Amberlite XAD-2 column, which was washed with water and eluted with methanol. The eluate was concentrated to about 0.5 mL under vacuum at 35°C, and then measured by liquid chromatography and UV detection. Two analytical columns were used for confirmation. The average recoveries of OTC, TC, and CTC from meat and fish fortified at 1, 1, and 3 ppm were 82.6, 81.5, and 67.0% respectively.


1995 ◽  
Vol 78 (1) ◽  
pp. 80-82 ◽  
Author(s):  
Hyoung S Lee

Abstract An interlaboratory study was carried out for the determination of benzoic acid in orange juice by liquid chromatography. The orange juice was fortified with 0.5–10 ppm benzoic acid. Statistical analysis of the results showed that relative reproducibility (RSDR) between laboratories ranged from 6.92 to 15.97% for juice fortified with 1-10 ppm benzoic acid; RSDr was 27.90% for juice fortified with 0.5 ppm benzoic acid. Mean recoveries ranged from 94.5% for 4 ppm benzoic acid to 114% for 0.5 ppm benzoic acid. Total variability increased with increasing fortification level as measured by standard deviation for reproducibility (SR).


1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.


1979 ◽  
Vol 62 (1) ◽  
pp. 171-175 ◽  
Author(s):  
Alfred F Haeberer ◽  
Orestes T Chortyk

Abstract A method is presented for the determination of the plant growth regulator maleic hydrazide (MH; l,2-dihydro-3,6-pyridazinedione) in tobacco and tobacco smoke. Residues are converted to the bis(trimethylsilyl) derivative before analysis by gas-liquid chromatography. The method has been applied to cigarettes and condensed smoke and has been used to determine the per cent transfer of MH into cigarette smoke. Free MH residues could be determined directly on the tobacco samples, whereas total MH values were obtainable only after acid hydrolysis. In spite of large MH residues in tobacco, only 0.2% of the MH was transferred into smoke.


1980 ◽  
Vol 63 (1) ◽  
pp. 33-36
Author(s):  
Molly I Keating

Abstract A rapid method for the analysis of dip washes is described which eliminates the usual solvent extraction procedure. The dip wash is initially diluted with acetone and then with petroleum ether. The diluted dip wash is analyzed by gasliquid chromatography, using an alkali ionization detector sensitive to phosphorus compounds. The method was applied to the determination of dioxathion (2,3-ρ-dioxanedithiol S,S-bis(O,O-diethyl phosphorodithioate)), and quintiofos (O-ethyl O-8-quinolyl phenylphosphonothioate) dip washes. Average recoveries from fouled dip washes were 100 and 104%. GLC of these compounds with an internal standard is described, which improves the precision of the method to ±2%.


1977 ◽  
Vol 60 (6) ◽  
pp. 1307-1309 ◽  
Author(s):  
Hendrik J Bakker

Abstract Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively.


1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.


1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day

Abstract A residue method is described for determination of the aquatic herbicide fluridone (1-methy1-3-phenyl-5-[3-(trifluoromethyl)phenyl]-4(1H)- pyridinone) and its metabolite (1-methy1-3-(4-hydroxyphenyl)-5-[3- (trifluoromethyl)phenyl]-4(1H)-pyridinone) in fish and crayfish tissues. Both compounds are extracted from tissues with methanol, and the extracts are subjected to acidic hydrolysis to release conjugated forms of fluridone and the metabolite. Sample extracts are purified by liquidliquid partitioning and Florisil Sep-Pak® column chromatography. Both compounds are separated and measured by reverse phase liquid chromatography with UV detection at 313 nm. In the absence of interfering peaks, the method has a detection limit of approximately 0.04 ppm of either compound. Overall, recoveries averaged 96% for fluridone and 78% for the metabolite for all tissue types combined.


1995 ◽  
Vol 78 (3) ◽  
pp. 841-845 ◽  
Author(s):  
Bertil Lindgren ◽  
Tomas Berglöf ◽  
Åsa Ramberg ◽  
Anna Stepdmska ◽  
Malin Åkerblom

Abstract A method is presented for rapid determination of bromide ion in commodities and blood by paired-ion liquid chromatography with electrochemical detection. The method involves extraction of samples with water and filtration. Blood is passed through a Sep-Pak C18 minicolumn. Recoveries are usually close to 100%, with satisfactory precision. The detection limit is 1 mg/kg. The method needs little labor and uses no noxious solvents or reagents.


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